| 稳定同位素标记D_4-罗丹明B的合成及表征 |
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| 引用本文： | 王浩然,杨维成,涂亚辉,杨超,方超,李美华,罗勇,吴范宏. 稳定同位素标记D_4-罗丹明B的合成及表征[J]. 应用化学, 2016, 33(8): 939-944. DOI: 10.11944/j.issn.1000-0518.2016.08.150374 |
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| 作者姓名： | 王浩然 杨维成 涂亚辉 杨超 方超 李美华 罗勇 吴范宏 |
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| 作者单位： | 上海应用技术学院 上海 201418; 上海化工研究院 上海 200062; 国家同位素工程技术研究中心-上海分中心 上海 200062 |
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| 基金项目： | 国家科技支撑计划(2015BAK45B01-20)资助项目 |
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| 摘 要： | 以全氘代邻二甲苯为同位素标记前体,经氧化得到的D_4-邻苯二甲酸与3-羟基-N,N-二乙基苯胺反应生成稳定同位素标记的D_4-罗丹明B,总收率36.9%。目标产物的结构经质谱(MS)、核磁(NMR)等技术手段表征确认,通过高效液相色谱确定化学纯度高于98.0%,同位素氘丰度大于98.0%。将其作为同位素内标试剂用于果汁中罗丹明B的残留检测,在0.05~50 mg/L范围内呈良好的线性关系,其检出限为5μg/kg,回收率为96.4%~103.4%,相对标准偏差(RSD)为1.0%~1.2%,具有很高的灵敏度和准确性。为食品安全领域违禁色素的检测提供了一种可靠实用的方法。
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| 关 键 词： | 稳定同位素标记 D4-罗丹明B 合成 内标 食品安全 |
| 收稿时间： | 2015-10-21 |
Synthesis and Properties of Stable Isotope Deuterium Labeled D4-Rhodamine B |
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| WANG Haoran,YANG Weicheng,TU Yahui,YANG Chao,FANG Chao,LI Meihua,LUO Yong,WU Fanhong. Synthesis and Properties of Stable Isotope Deuterium Labeled D4-Rhodamine B[J]. Chinese Journal of Applied Chemistry, 2016, 33(8): 939-944. DOI: 10.11944/j.issn.1000-0518.2016.08.150374 |
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| Authors: | WANG Haoran YANG Weicheng TU Yahui YANG Chao FANG Chao LI Meihua LUO Yong WU Fanhong |
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| Affiliation: | School of Chemical and Environmental Engineering, Shanghai Institute of Technology,Shanghai 201418,China; Shanghai Research Institute of Chemical Industry,Shanghai 200062,China; National Isotope Engineering Technology Research Center-Shanghai Sub-Center,Shanghai 200062,China |
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| Abstract: | This paper presents an efficient synthesis of stable isotope labeled D4-rhodamine B from deuterated orthoxylene through oxidation and its reaction with 3-diethylaminophenol in 36.9% total yield. The deuterated product was confirmed by mass spectrometry(MS) and nuclear magnetic resonance(NMR). Its chemical purity is higher than 98.0% by high performance liquid chromatography(HPLC), and isotopic enrichment is higher than 98.0%(atom D). D4-rhodamine B was used as internal standard for the determination of rhodamine B in orange juice with linear calibration curve of 0.05~50 mg/L, limit for determination of 5 μg/kg, recovery of 96.4%~103.4% and relative standard deviation(RSD) of 1.0%~1.2%. This method is proved to be accurate and sensitive for the determination of rhodamine in food safety. |
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| Keywords: | stable isotope-labeling D4-rhodamine B synthesis internal standard food safety |
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